Agilent Technologies 5800 ICP-OES User manual

Agilent 5800 and 5900 ICP-OES
User's Guide

2 Agilent 5800 and 5900 ICP-OES User's Guide
Notices
Manual Part Number
G8020-90002
Edition 1, October 2019
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© Agilent Technologies, Inc. 2019
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Safety Notices
A CAUTION notice denotes a hazard. It
calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
A WARNING notice denotes a hazard. It
calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in personal injury or death.
Do not proceed beyond a WARNING
notice until the indicated conditions are
fully understood and met.
WARNING
CAUTION

Contents
Agilent 5800 and 5900 ICP-OES User's Guide 3
Contents
1Safety Practices and Hazards 7
General 7
Verifying Safe State 8
Plasma 8
Heat, Vapors and Fumes 9
Compressed Gas Hazards 9
Electrical Hazards 10
Other Precautions 11
Warning Symbols 12
2Introduction 15
Site Preparation Requirements 15
User Documentation 15
Conventions 16
Notes and tips 16
ICP-OES Argon Gas Supply 16
Exhaust System 17
ICP-OES Instrument Cooling Air Supply 17
Water Chiller System 18
Drain Vessel 18
3Installation 19
Agilent ICP-OES Instrument Overview 20
Instrument Status LED Color Coding 22
Front Power On/Off Button 22
ICP Expert Software 23
Connecting ICP Expert software to the ICP-OES 24

Contents
4 Agilent 5800 and 5900 ICP-OES User's Guide
Performing a Detector and Wavelength Calibration 24
Saving and viewing the calibration data 25
Hardware Components Replacement 25
ICP-OES torches 26
Torch Assembly and Disassembly 27
Assembly of the semi-demountable torch 28
Assembly of the fully demountable torch 31
Torch disassembly 32
Accessories 35
SPS 4 35
Advanced Valve System (AVS) — AVS 4, AVS 6 and AVS 7 36
External Inlet Duct Adapter 36
Vapor Generation Accessory (VGA) 36
Multimode Sample Introduction System (MSIS) 36
Argon Humidifier 37
IsoMist Programmable Temperature Spray Chamber 37
4Operation 39
Analysis Checklist 39
Turning On the Instrument and Software 40
Turning on the instrument for the first time (or from long term
shutdown) 40
Running the instrument from standby 41
Preparing for Analysis 41
Performing a Detector and Wavelength Calibration 42
Creating/Opening a Worksheet 42
Creating a new worksheet 42
Opening an existing worksheet 43

Contents
Agilent 5800 and 5900 ICP-OES User's Guide 5
Creating a new worksheet from a template 43
Developing a Method 43
Running Samples 45
Printing a Report 45
Turning Off the Instrument 46
Instrument Standby Mode with argon on 46
Instrument Standby Mode with argon off 46
Setting the instrument to Standby Mode with argon on or off 47
Turning off the instrument for long term shutdown 48
5Maintenance and Troubleshooting 51
Routine 52
Cleaning 54
Torch Cleaning 54
Important 55
Acid soak cleaning procedure for the torch for aqueous or acid-based
samples (one piece and semi-demountable torches) 56
Rinsing the torch 59
Drying the torch 61
Additional checks after cleaning 62
Troubleshooting 63
Spare Parts 63
Technical Support 64

Contents
6 Agilent 5800 and 5900 ICP-OES User's Guide
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Safety Practices and Hazards
Agilent 5800 and 5900 ICP-OES User's Guide 7
1Safety Practices and Hazards
General 7
Verifying Safe State 8
Plasma 8
Heat, Vapors and Fumes 9
Compressed Gas Hazards 9
Electrical Hazards 10
Other Precautions 11
Warning Symbols 12
General
Unless otherwise specified, statements in this manual apply to both the Agilent
5800 and 5900 ICP-OES instruments.
Operation of an Agilent ICP-OES involves the use of compressed gases, high
voltage radio frequency energy and hazardous materials including corrosive fluids
and flammable liquids. Careless, improper or unskilled use of this spectrometer or
chemicals used with it can cause death or serious injury to personnel, and/or
severe damage to equipment and property. Only trained personnel should use this
instrument.
The spectrometer incorporates interlocks and covers that are designed to prevent
inadvertent contact with any potential hazards. If the instrument is used in any
manner not specified by Agilent, this protection provided by the equipment may be
impaired. It is good practice to develop safe working habits that do not depend
upon the correct operation of the interlocks for safe operation. It is essential that
no interlock or cover is bypassed, damaged or removed.
The safety practices described below are provided to help the user operate the
instrument safely. Read each safety topic thoroughly before attempting to operate
the instrument and always operate the spectrometer in accordance with these
safety practices.

Safety Practices and Hazards
8 Agilent 5800 and 5900 ICP-OES User's Guide
Verifying Safe State
The following general safety precautions must be observed during all phases of
operation, maintenance and service of this instrument.
To ensure continued safety of the instrument after maintenance or service
procedures verify the instrument is returned to a safe state for the user. This
includes running performance checks to verify the instruments safety systems are
functioning correctly. Check the general condition of the instrument during
operation for wear or signs of corrosion that are likely to inhibit function or safety.
Failure to comply with these precautions or with specific warnings elsewhere in
this manual violates safety standards of design, manufacture, and intended use of
the instrument. Agilent Technologies assumes no liability for the customer’s
failure to comply with these requirements.
Plasma
The plasma is extremely hot (about 10,000 °C) and radiates dangerous levels of
radio frequency (RF) and ultraviolet (UV) energy. The work coil operates at 1,500 V
RMS and about 27 MHz. Exposure to the RF and UV energy can cause severe skin
damage and cataracts of the eyes, while close contact with the operating plasma
can result in severe heat burns to the skin, and an electrical discharge that can
jump a considerable distance and may cause death, severe electric shock or sub-
surface skin burns.
The plasma must never be operated unless:
the plasma compartment door is closed, with the door handle fully closed; and
the space above the chimney and air intake is clear of objects.
The shielding around the torch compartment is designed to reduce UV, visible and
RF radiation to safe levels while still permitting easy access to, as well as
installation and viewing of, the torch. The spectrometer has an interlock system
that is designed to extinguish the plasma if the mains supply fails, the handle on
the torch compartment door is opened, or the torch loading handle is open. Do not
attempt to bypass the interlock system.

Safety Practices and Hazards
Agilent 5800 and 5900 ICP-OES User's Guide 9
Before opening the torch compartment door, always extinguish the plasma by
pressing SHIFT + F5 on the keyboard or by clicking the ‘Plasma Off’ icon on the
ICP Expert software toolbar.
The torch and its surroundings remain hot for up to five minutes after the plasma
is extinguished. Touching this area before it has cooled sufficiently may result in
burns. Allow the torch and torch compartment to cool before carrying out any
work in this area, or wear heat-resistant gloves.
The plasma system has been carefully designed to operate safely and effectively
when using torches and related components that conform to Agilent’s design
criteria. Use of non-approved components in the plasma compartment may render
the system inoperative and/or hazardous. It may also invalidate the warranty on
the instrument. Use only torches and related components supplied or authorized
by Agilent.
Heat, Vapors and Fumes
Heat, ozone, vapors and fumes generated by the plasma can be hazardous and
must be extracted from the instrument by means of an exhaust system. Ensure
that an exhaust system of the appropriate type is fitted (as specified in the Site
Preparation Guide). The system must be vented to the outside air in accordance
with local regulations and never within the building. Regularly check the exhaust
system by smoke test to ensure that the exhaust system is functioning correctly.
The exhaust system must always be switched on before igniting the plasma.
Compressed Gas Hazards
All compressed gases (other than air) can create a hazard if they leak into the
atmosphere. Even small leaks in gas supply systems can be dangerous. Any leak
(except that of air or oxygen) can result in an oxygen-deficient atmosphere, which
can cause asphyxiation. The area in which cylinders are stored and the area
surrounding the instrument must be adequately ventilated to prevent such gas
accumulations.

Safety Practices and Hazards
10 Agilent 5800 and 5900 ICP-OES User's Guide
Gas cylinders must be stored and handled strictly in accordance with local safety
codes and regulations. Cylinders must be used and stored only in a vertical
position and secured to an immovable structure or a properly constructed cylinder
stand. Move cylinders only by securing them to a properly constructed trolley.
Use only approved regulator and hose connectors (refer to the gas supplier’s
instructions). Keep gas cylinders cool and properly labeled. (All cylinders are fitted
with a pressure relief device that will rupture and empty the cylinder if the internal
pressure is raised above the safe limit by excessive temperatures.) Ensure that
you have the correct gas before connecting it to the instrument.
The primary gas used with the spectrometer is argon, which is the conductive gas
for the plasma. Argon or nitrogen can be used as the polychromator purge gas.
Other gases may be required for future options and accessories. Use only
‘instrument grade’ gases with your spectrometer.
If using cryogenic gases (for example, liquid argon), prevent severe burns by
wearing suitable protective clothing and gloves.
Electrical Hazards
The spectrometer system and some accessories contain electrical circuits,
devices and components operating at dangerous voltages. Contact with these
circuits, devices and components can cause death, serious injury or painful
electric shock. Panels or covers which are retained by screws on the spectrometer
and accessories may be opened only by Agilenttrained, Agilent-qualified or
Agilentapproved field service engineers (unless specified otherwise). Consult the
manuals or product labels supplied with your personal computer (PC), monitor,
printer and water-cooling system to determine which parts of those systems are
operator-accessible.
Connecting the Agilent ICP-OES to a power source that is not equipped with a
protective earth contact creates a shock hazard for the operator and can damage
the instrument. Likewise, interrupting the protective conductor inside or outside
the Agilent ICP-OES or defeating the power cord ground creates a shock hazard
for the operator and can damage the instrument.

Safety Practices and Hazards
Agilent 5800 and 5900 ICP-OES User's Guide 11
Other Precautions
Use of the spectrometer system and accessories may involve materials, solvents
and solutions which are flammable, corrosive, toxic or otherwise hazardous.
Careless, improper or unskilled use of such materials, solvents and solutions can
create explosion hazards, chemical burn hazards, fire hazards, toxicity and other
hazards that can result in death, serious personal injury or damage to equipment.
Apply all necessary precautions including use of lab coats, safety goggles and
other appropriate forms of personal protection. All wastes should be disposed of
in accordance with local regulatory requirements.
Operation of an ICP-OES involves analysis of solutions that have been prepared in
or digested with acids, or in some cases, samples that have been prepared in
organic solvents.
In case of uncertainty about a specific fluid, that fluid should not be used until
confirmation by the manufacturer that it will not present a hazard.
The acid concentration in the sample that is measured varies, depending upon the
digestion steps and acid types used. Instrument users should be aware of the
hazards associated with use of the acids used for sample preparation and apply
all necessary precautions including use of lab coats, safety goggles and other
appropriate forms of personal protection. The acid wastes should be disposed of
in accordance with local regulatory requirements.
The type, volatility and concentration of the organic solvents used in the sample
that is measured varies, depending upon the selected solvent and the sample
preparation involved. Instrument users should be aware of the hazards associated
with use of the organic solvents for sample preparation, and apply all necessary
precautions including ensuring adequate ventilation during use, and use of lab
coats, safety goggles, gloves and other appropriate forms of personal protection.
The organic wastes should be disposed of in accordance with local regulatory
requirements.
Air flow to the air intake port of the spectrometer and accessories must be
unobstructed. Do not block the ventilation grills on the spectrometer and
accessories. Consult the manuals supplied with your PC, monitor, printer and
water-cooling system for their specific ventilation requirements.
Great care should be taken when working with glass or quartz parts to prevent
breakage and cuts. This is especially important when inserting the nebulizer into
the spray chamber or removing and replacing pieces of broken torch.

Safety Practices and Hazards
12 Agilent 5800 and 5900 ICP-OES User's Guide
The spectrometer weighs approximately 90 kg (200 lb). To avoid injury to
personnel or damage to the instrument or property, always use suitable
mechanical lifting device to move the instrument.
Use only Agilent-supplied or approved spares with your instrument Only trained
operators should use the instrument.
Warning Symbols
The following is a list of symbols that may appear in conjunction with warnings in
this manual or on the spectrometer. The hazard they describe is also shown. The
beginning of the warning text is noted by a warning icon:
WARNING
A triangular symbol indicates a warning. The meanings of the symbols that may
appear alongside warnings in the documentation or on the instrument itself are as
follows:
Broken glass Chemical hazard
Disconnect power
Electrical shock
Extreme cold hazard
Eye hazard
Fire hazard
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
Hot surface Noxious gases
RF radiation

Safety Practices and Hazards
Agilent 5800 and 5900 ICP-OES User's Guide 13
The following symbol may be used on warning labels attached to the instrument.
When you see this symbol, refer to the relevant operation or service manual for the
correct procedure referred to by that warning label.
The following symbols appear on the instrument for your information.
I Mains power on
0 Mains power off
Single phase alternating current
Protective ground terminal.
Socket for Agilent accessory serial cable
Socket for Ethernet LAN cable
Socket for Agilent accessory USB cable
Indication of correct orientation of gas filter flow direction
Caution, disconnect all supplies, risk of electric shock

Safety Practices and Hazards
14 Agilent 5800 and 5900 ICP-OES User's Guide
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Introduction
Agilent 5800 and 5900 ICP-OES User's Guide 15
2Introduction
Site Preparation Requirements 15
User Documentation 15
ICP-OES Argon Gas Supply 16
Exhaust System 17
ICP-OES Instrument Cooling Air Supply 17
Water Chiller System 18
Drain Vessel 18
Site Preparation Requirements
Prior to receiving your instrument, you will have been provided with an Agilent
5800 and 5900 ICP-OES Site Preparation Guide, which describes the
environmental and operating requirements of the ICP-OES system. You must
prepare your laboratory according to these instructions before the ICP-OES can be
installed. You should keep the Site Preparation Guide for future reference for
example, if you plan to move your instrument. If you have misplaced your copy,
you can obtain a free replacement from your local Agilent office.
Position the equipment for easy access to the disconnecting switch on the left
side of the instrument.
User Documentation
You have been provided with the following documentation to help you set up and
operate your Agilent ICP-OES system:
This User’s Guide, with safety practices and hazards information, instructions
for finding information about installing and maintaining the components of the
ICP-OES and a brief operation overview.

Introduction
16 Agilent 5800 and 5900 ICP-OES User's Guide
An extensive Help and Learning Center containing context-sensitive Help with
information on how to set up methods and run instrument tests, hardware
basics and maintenance videos, step-by-step instructions for frequently
performed operations and instructions for using any accessories you ordered.
Conventions
The following conventions have been used throughout the documentation:
Menu items, menu options and field names (for example, click Copy from the
Edit menu) have been typed in bold. Bold is also used to signify the buttons
appearing throughout the software (e.g., click OK).
ALL CAPITALS indicate keyboard commands (e.g., press the F2 key) and text
you must type in from the keyboard (e.g., type SETUP at the prompt).
Notes and tips
A Note is used to give advice or information.
A Tip is used to give practical hints to help you achieve the best possible
performance from your ICP-OES.
ICP-OES Argon Gas Supply
Table 1. Typical flow rates for the Agilent ICP-OES instruments
Typical Flows Argon (with nitrogen purge gas)
Measuring wavelengths
> 189 nm (poly boost off)
Argon flow 16.7 L/min
Nitrogen flow 0.8 L/min
Measuring wavelengths
< 189 nm (poly boost on)
Argon flow 16.7 L/min
Nitrogen flow 4.4 L/min
Argon can be used as a plasma gas and purge gas which results in a higher total
argon flow rate.
The user (or other authorized personnel) must carry out appropriate leak tests
necessary to ensure safety on the gas and liquid connections that the operator is
directed to assemble during installation, normal use or maintenance.

Introduction
Agilent 5800 and 5900 ICP-OES User's Guide 17
Exhaust System
The plasma operates at extremely high temperatures. The ICP-OES instrument
exhaust fumes can be noxious or corrosive.
The exhaust system should be checked regularly to ensure adequate flow. Consult
the ICP-OES Site Prep Guide for the appropriate flow rates.
WARNING
Hot Surface
The external vent may become hot during ICP-OES instrument operation
and remain hot for some time after the instrument has been switched off.
Allow the external vent to cool for at least five minutes before attempting
to remove the exhaust hose. Use heat-resistant gloves.
ICP-OES Instrument Cooling Air Supply
The ICP-OES instrument requires clean, dry, non-corrosive air for cooling purposes.
This is supplied to the instrument through an air supply vent located at the top, left
of the instrument. The vent has a dust filter, to filter out particulate matter.
The air supply is used to cool the internal mechanical and electronic components
of the instrument. Several of these assemblies contain parts prone to corrosion.
The introduction of cooling air contaminated with high levels of acid vapors or
other corrosive substances may cause damage to the instrument.
Due to the corrosive nature of some analytical work, it is recommended that in
applications demanding high usage of corrosive materials, an external cooling air
supply system is provided. It is required that the cooling air be supplied from an
environmentally-controlled area that is away from the instrument exhaust and any
other area where corrosive materials are stored or used. Do not duct humid, warm
air into an instrument in a cooled laboratory environment.
The cooling air system with flue, fan, ducting and supply cowl, must provide
positive air pressure at the instrument inlet of 4 m3/min (141 ft3/min) when using
the External Inlet Duct Adaptor Kit. The ducting should be corrosion-resistant and
fire-proof.

Introduction
18 Agilent 5800 and 5900 ICP-OES User's Guide
Water Chiller System
Agilent ICP-OES instruments require a source of cooling water. Refer to the Site
Preparation Guide for compatible water chilling systems and to the documentation
provided with the water chilling system for installation and use instructions.
NOTE Pressure regulation is recommended for supplies where the cooling water
pressure may be subject to fluctuations. Pressure regulation is necessary for
supplies that may exceed the maximum permissible pressure of 400 kPa (58 psi).
The instrument is equipped with a water flow sensor, which will stop operation of the
plasma if the cooling water flow through the instrument drops below 1.7 L/min (0.45
gpm). A second water flow sensor will stop the camera Peltier cooling assembly if the
water flow through the instrument drops below 0.2 L/min (0.05 gpm).
CAUTION Always ensure the water chillersystem is on before igniting the plasma.
Drain Vessel
The Agilent ICP-OES system needs a drain vessel for disposal of excess fluids
from the spray chamber or autosampler. Suitable tubing is supplied with the
spectrometer for use with inorganic solvents. When using organic solvents,
different drain tubing that is suitable for the solvent in use will be required.
A chemically inert container, not glass or of a narrow-necked style, to hold a
minimum of 2 liters (4 pints) of waste must be provided by the user. It should be
located underneath the sample compartment (or on the right side of the
instrument), where it is protected by the bench and in full view of the operator.

Installation
Agilent 5800 and 5900 ICP-OES User's Guide 19
3Installation
Agilent ICP-OES Instrument Overview 20
Instrument Status LED Color Coding 22
Front Power On/Off Button 22
ICP Expert Software 23
Connecting ICP Expert software to the ICP-OES 24
Performing a Detector and Wavelength Calibration 24
Hardware Components Replacement 25
Torch Assembly and Disassembly 27
Accessories 35
The Agilent ICP-OES must be installed by an Agilent-trained, Agilent-qualified or
Agilent-authorized field service engineer.
You should have completed and returned the form in the Site Preparation Guide
stating that you have prepared the laboratory in accordance with the requirements
detailed in that manual. An Agilent representative will then arrange a suitable
installation date with you.
Details for unpacking the instrument and what to do in case it has been damaged
in transit are also outlined in the Site Preparation Guide.

Installation
20 Agilent 5800 and 5900 ICP-OES User's Guide
Agilent ICP-OES Instrument Overview
Figure 1. Front and side of the ICP-OES instrument
1. Exhaust 8. Torch loader handle 15. Torch compartment handle
2. Air inlet filter 9. Spray chamber 16. Water inlet assembly
3. Pre-optics cone and axial
viewing window (not shown)
10. Nebulizer 17. Optics purge filter for argon or
nitrogen
4. Snout and radial viewing
window (not shown)
11. Peristaltic pump 18. Gas supply assembly
5. Work coil 12. Mains power switch and
cable connection
19. Optional AVS 4, AVS 6 or AVS 7
Switching Valve accessory location
6. Torch 13. Front panel power button 20. Drain for liquid overflow
7. Nebulizer and make up gas
connections
14. LED instrument status
indicator
11
7
9
10
8
1
14
2
5
3
18
15
16
17
6
13
12
20
4
19